data_shelx _audit_creation_method 'SHELXL-2018/1' _shelx_SHELXL_version_number '2018/1' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Al0.06 H18 Ca0.38 Fe2.21 Mg0.29 Mn2.45 Na0.62 O26 P4' _chemical_formula_weight 850.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mn' 'Mn' 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ca' 'Ca' 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 13 _space_group_name_H-M_alt 'P 1 2/a 1' _space_group_name_Hall '-P 2ya' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, -y, z' _cell_length_a 15.1359(10) _cell_length_b 7.2035(3) _cell_length_c 9.9876(6) _cell_angle_alpha 90 _cell_angle_beta 110.361(5) _cell_angle_gamma 90 _cell_volume 1020.92(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2077 _cell_measurement_theta_min 3.5290 _cell_measurement_theta_max 25.8690 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.766 _exptl_crystal_F_000 843 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.075 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 3.561 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89863 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1695 _diffrn_reflns_number 33511 _diffrn_reflns_av_unetI/netI 0.0795 _diffrn_reflns_av_R_equivalents 0.1577 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.553 _diffrn_reflns_theta_max 27.877 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measured_fraction_theta_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_point_group_measured_fraction_full 0.986 _reflns_number_total 2406 _reflns_number_gt 1587 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+12.8852P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refxyz _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 2406 _refine_ls_number_parameters 199 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1490 _refine_ls_wR_factor_gt 0.1215 _refine_ls_goodness_of_fit_ref 0.862 _refine_ls_restrained_S_all 0.860 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group NaX Na 0.250000 0.9726(3) 0.000000 0.0108(6) Uani 0.62 2 d S T P . . CaX Ca 0.250000 0.9726(3) 0.000000 0.0108(6) Uani 0.38 2 d S T P . . Mn1 Mn 0.250000 0.4769(2) 0.000000 0.0115(5) Uani 0.68 2 d S T P . . Fe1 Mn 0.250000 0.4769(2) 0.000000 0.0115(5) Uani 0.32 2 d S T P . . Mn2A Mn 0.500000 0.000000 0.500000 0.0181(4) Uani 0.716 2 d S . P . . Fe2A Fe 0.500000 0.000000 0.500000 0.0181(4) Uani 0.142 2 d S . P . . Mg2A Mg 0.500000 0.000000 0.500000 0.0181(4) Uani 0.142 2 d S . P . . Mn2B Mn 0.250000 0.4986(2) 0.500000 0.0138(4) Uani 0.718 2 d S T P . . Fe2B Fe 0.250000 0.4986(2) 0.500000 0.0138(4) Uani 0.136 2 d S T P . . Mg2B Mg 0.250000 0.4986(2) 0.500000 0.0138(4) Uani 0.146 2 d S T P . . Fe3A Fe 0.000000 0.000000 0.000000 0.0102(3) Uani 0.766 2 d S . P . . Mn3A Mn 0.000000 0.000000 0.000000 0.0102(3) Uani 0.21 2 d S . P . . Al3A Al 0.000000 0.000000 0.000000 0.0102(3) Uani 0.026 2 d S . P . . Fe3B Fe 0.000000 0.500000 0.000000 0.0104(4) Uani 0.846 2 d S . P . . Mn3B Mn 0.000000 0.500000 0.000000 0.0104(4) Uani 0.12 2 d S . P . . Al3B Al 0.000000 0.500000 0.000000 0.0104(4) Uani 0.034 2 d S . P . . P1 P 0.18453(12) 0.2616(2) 0.18428(18) 0.0096(6) Uani 1 1 d . . . . . P2 P 0.08131(12) 0.7451(2) 0.79812(18) 0.0086(6) Uani 1 1 d . . . . . O1 O 0.2766(3) 0.2398(8) 0.1505(5) 0.0254(13) Uani 1 1 d . . . . . O2 O 0.2051(4) 0.2960(7) 0.3414(5) 0.0219(12) Uani 1 1 d . . . . . O3 O 0.1255(3) 0.0893(7) 0.1360(5) 0.0239(12) Uani 1 1 d . . . . . O4 O 0.1385(3) 0.4323(6) 0.0875(5) 0.0144(10) Uani 1 1 d . . . . . O5 O 0.1863(3) 0.6884(7) 0.8584(5) 0.0209(12) Uani 1 1 d . . . . . O6 O 0.0538(4) 0.7758(7) 0.6392(5) 0.0209(11) Uani 1 1 d . . . . . O7 O 0.0730(4) 0.9247(7) 0.8760(5) 0.0218(12) Uani 1 1 d . . . . . O8 O 0.0209(3) 0.5903(6) 0.8260(5) 0.0183(11) Uani 1 1 d . . . . . OH9 O 0.0269(3) 0.7503(6) 0.0954(5) 0.0153(10) Uani 1 1 d D . . . . OW10 O 0.2247(4) 0.7250(8) 0.3384(6) 0.0307(14) Uani 1 1 d D . . . . OW11 O 0.4491(4) 0.2185(8) 0.3401(6) 0.0360(15) Uani 1 1 d D . . . . OW12 O 0.6333(4) 0.9908(8) 0.4600(7) 0.0341(14) Uani 1 1 d D . . . . OW13 O 0.3951(4) 0.5115(8) 0.5140(6) 0.0274(13) Uani 1 1 d D . . . . H9 H 0.015(7) 0.743(14) 0.169(6) 0.050 Uiso 1 1 d D U . . . H10A H 0.253(5) 0.731(14) 0.284(8) 0.050 Uiso 1 1 d D U . . . H10B H 0.170(2) 0.743(14) 0.298(8) 0.050 Uiso 1 1 d D U . . . H11A H 0.393(3) 0.226(13) 0.292(8) 0.050 Uiso 1 1 d D U . . . H11B H 0.455(6) 0.285(12) 0.409(6) 0.050 Uiso 1 1 d D U . . . H12A H 0.642(6) 0.910(10) 0.409(7) 0.050 Uiso 1 1 d D U . . . H12B H 0.675(5) 0.984(13) 0.536(5) 0.050 Uiso 1 1 d D U . . . H13A H 0.416(6) 0.594(10) 0.475(8) 0.050 Uiso 1 1 d D U . . . H13B H 0.436(5) 0.506(13) 0.595(5) 0.050 Uiso 1 1 d D U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 NaX 0.0139(13) 0.0009(12) 0.0115(13) 0.000 -0.0034(11) 0.000 CaX 0.0139(13) 0.0009(12) 0.0115(13) 0.000 -0.0034(11) 0.000 Mn1 0.0098(8) 0.0120(8) 0.0139(8) 0.000 0.0058(6) 0.000 Mn2A 0.0169(8) 0.0134(8) 0.0216(9) -0.0058(7) 0.0038(7) -0.0007(7) Fe2A 0.0169(8) 0.0134(8) 0.0216(9) -0.0058(7) 0.0038(7) -0.0007(7) Mg2A 0.0169(8) 0.0134(8) 0.0216(9) -0.0058(7) 0.0038(7) -0.0007(7) Mn2B 0.0143(8) 0.0148(8) 0.0136(8) 0.000 0.0067(6) 0.000 Fe2B 0.0143(8) 0.0148(8) 0.0136(8) 0.000 0.0067(6) 0.000 Mg2B 0.0143(8) 0.0148(8) 0.0136(8) 0.000 0.0067(6) 0.000 Fe3A 0.0082(7) 0.0063(7) 0.0163(7) -0.0019(5) 0.0047(5) -0.0001(5) Mn3A 0.0082(7) 0.0063(7) 0.0163(7) -0.0019(5) 0.0047(5) -0.0001(5) Al3A 0.0082(7) 0.0063(7) 0.0163(7) -0.0019(5) 0.0047(5) -0.0001(5) Fe3B 0.0085(7) 0.0069(7) 0.0181(7) -0.0001(5) 0.0076(6) -0.0001(5) Mn3B 0.0085(7) 0.0069(7) 0.0181(7) -0.0001(5) 0.0076(6) -0.0001(5) Al3B 0.0085(7) 0.0069(7) 0.0181(7) -0.0001(5) 0.0076(6) -0.0001(5) P1 0.0062(9) 0.0101(10) 0.0116(9) -0.0021(7) 0.0019(6) 0.0003(7) P2 0.0075(9) 0.0088(9) 0.0095(9) 0.0008(7) 0.0030(7) 0.0009(7) O1 0.016(3) 0.042(3) 0.018(3) 0.003(2) 0.007(2) 0.011(2) O2 0.030(3) 0.022(3) 0.016(3) -0.007(2) 0.011(2) -0.002(2) O3 0.021(3) 0.011(2) 0.028(3) 0.000(2) -0.006(2) -0.003(2) O4 0.011(2) 0.012(2) 0.022(3) 0.001(2) 0.008(2) 0.0020(19) O5 0.011(2) 0.032(3) 0.021(3) 0.001(2) 0.007(2) 0.010(2) O6 0.033(3) 0.016(3) 0.012(2) 0.003(2) 0.006(2) 0.005(2) O7 0.032(3) 0.014(2) 0.027(3) -0.001(2) 0.019(2) -0.002(2) O8 0.020(3) 0.010(2) 0.029(3) -0.001(2) 0.014(2) -0.004(2) OH9 0.017(2) 0.008(2) 0.024(3) 0.000(2) 0.011(2) -0.0005(19) OW10 0.039(3) 0.030(3) 0.031(3) 0.008(3) 0.023(3) 0.013(3) OW11 0.037(3) 0.028(3) 0.025(3) -0.002(3) -0.012(3) -0.007(3) OW12 0.028(3) 0.032(4) 0.045(4) -0.013(3) 0.017(3) -0.005(3) OW13 0.015(3) 0.030(3) 0.038(3) 0.008(3) 0.010(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag NaX O1 2.389(6) 1_565 ? NaX O1 2.389(6) 2_565 ? NaX O5 2.484(6) 2_556 ? NaX O5 2.484(6) 1_554 ? NaX O7 2.554(5) 1_554 ? NaX O7 2.554(5) 2_556 ? NaX O3 2.808(6) 2_565 ? NaX O3 2.808(6) 1_565 ? Mn1 O5 2.074(5) 1_554 ? Mn1 O5 2.074(5) 2_556 ? Mn1 O4 2.178(4) . ? Mn1 O4 2.178(4) 2 ? Mn1 O1 2.218(5) . ? Mn1 O1 2.218(5) 2 ? Mn2A O6 2.101(5) 4_665 ? Mn2A O6 2.101(5) 2_546 ? Mn2A OW11 2.183(6) 3_656 ? Mn2A OW11 2.183(6) . ? Mn2A OW12 2.190(6) 3_666 ? Mn2A OW12 2.190(6) 1_545 ? Mn2B O2 2.086(5) 2_556 ? Mn2B O2 2.086(5) . ? Mn2B OW13 2.154(5) . ? Mn2B OW13 2.154(5) 2_556 ? Mn2B OW10 2.232(6) 2_556 ? Mn2B OW10 2.232(6) . ? Fe3A O7 2.000(5) 3_566 ? Fe3A O7 2.000(5) 1_544 ? Fe3A OH9 2.010(5) 3_565 ? Fe3A OH9 2.010(5) 1_545 ? Fe3A O3 2.017(5) 3 ? Fe3A O3 2.017(5) . ? Fe3B O8 1.982(5) 3_566 ? Fe3B O8 1.982(5) 1_554 ? Fe3B OH9 2.014(5) . ? Fe3B OH9 2.014(5) 3_565 ? Fe3B O4 2.030(4) 3_565 ? Fe3B O4 2.030(4) . ? P1 O3 1.507(5) . ? P1 O2 1.510(5) . ? P1 O1 1.551(5) . ? P1 O4 1.570(5) . ? P2 O6 1.511(5) . ? P2 O8 1.527(5) . ? P2 O7 1.537(5) . ? P2 O5 1.546(5) . ? OH9 H9 0.82(3) . ? OW10 H10A 0.80(3) . ? OW10 H10B 0.80(3) . ? OW11 H11A 0.82(3) . ? OW11 H11B 0.82(3) . ? OW12 H12A 0.81(3) . ? OW12 H12B 0.80(3) . ? OW13 H13A 0.83(3) . ? OW13 H13B 0.83(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 NaX O1 72.6(3) 1_565 2_565 ? O1 NaX O5 111.02(17) 1_565 2_556 ? O1 NaX O5 165.79(16) 2_565 2_556 ? O1 NaX O5 165.79(16) 1_565 1_554 ? O1 NaX O5 111.02(17) 2_565 1_554 ? O5 NaX O5 69.0(2) 2_556 1_554 ? O1 NaX O7 109.43(17) 1_565 1_554 ? O1 NaX O7 83.40(16) 2_565 1_554 ? O5 NaX O7 107.37(17) 2_556 1_554 ? O5 NaX O7 58.60(15) 1_554 1_554 ? O1 NaX O7 83.40(16) 1_565 2_556 ? O1 NaX O7 109.43(17) 2_565 2_556 ? O5 NaX O7 58.60(15) 2_556 2_556 ? O5 NaX O7 107.37(17) 1_554 2_556 ? O7 NaX O7 164.5(2) 1_554 2_556 ? O1 NaX O3 93.93(17) 1_565 2_565 ? O1 NaX O3 56.56(16) 2_565 2_565 ? O5 NaX O3 109.23(15) 2_556 2_565 ? O5 NaX O3 99.44(15) 1_554 2_565 ? O7 NaX O3 124.99(15) 1_554 2_565 ? O7 NaX O3 60.49(14) 2_556 2_565 ? O1 NaX O3 56.56(16) 1_565 1_565 ? O1 NaX O3 93.93(17) 2_565 1_565 ? O5 NaX O3 99.44(15) 2_556 1_565 ? O5 NaX O3 109.23(15) 1_554 1_565 ? O7 NaX O3 60.49(14) 1_554 1_565 ? O7 NaX O3 124.99(15) 2_556 1_565 ? O3 NaX O3 145.2(2) 2_565 1_565 ? O1 NaX P2 138.81(13) 1_565 1_554 ? O1 NaX P2 95.51(12) 2_565 1_554 ? O5 NaX P2 90.19(13) 2_556 1_554 ? O5 NaX P2 29.43(11) 1_554 1_554 ? O7 NaX P2 29.42(11) 1_554 1_554 ? O7 NaX P2 136.79(14) 2_556 1_554 ? O3 NaX P2 112.44(10) 2_565 1_554 ? O3 NaX P2 86.19(10) 1_565 1_554 ? O1 NaX P2 95.51(12) 1_565 2_556 ? O1 NaX P2 138.81(13) 2_565 2_556 ? O5 NaX P2 29.43(11) 2_556 2_556 ? O5 NaX P2 90.19(13) 1_554 2_556 ? O7 NaX P2 136.79(14) 1_554 2_556 ? O7 NaX P2 29.42(11) 2_556 2_556 ? O3 NaX P2 86.19(10) 2_565 2_556 ? O3 NaX P2 112.44(10) 1_565 2_556 ? P2 NaX P2 116.47(10) 1_554 2_556 ? O1 NaX P1 28.40(12) 1_565 1_565 ? O1 NaX P1 79.46(14) 2_565 1_565 ? O5 NaX P1 110.46(12) 2_556 1_565 ? O5 NaX P1 137.47(11) 1_554 1_565 ? O7 NaX P1 83.26(11) 1_554 1_565 ? O7 NaX P1 107.18(12) 2_556 1_565 ? O3 NaX P1 118.95(13) 2_565 1_565 ? O3 NaX P1 28.50(10) 1_565 1_565 ? P2 NaX P1 111.81(5) 1_554 1_565 ? P2 NaX P1 108.82(5) 2_556 1_565 ? O1 NaX P1 79.46(14) 1_565 2_565 ? O1 NaX P1 28.40(12) 2_565 2_565 ? O5 NaX P1 137.47(11) 2_556 2_565 ? O5 NaX P1 110.46(12) 1_554 2_565 ? O7 NaX P1 107.18(12) 1_554 2_565 ? O7 NaX P1 83.26(11) 2_556 2_565 ? O3 NaX P1 28.50(10) 2_565 2_565 ? O3 NaX P1 118.95(13) 1_565 2_565 ? P2 NaX P1 108.82(5) 1_554 2_565 ? P2 NaX P1 111.81(5) 2_556 2_565 ? P1 NaX P1 97.51(9) 1_565 2_565 ? O5 Mn1 O5 85.5(3) 1_554 2_556 ? O5 Mn1 O4 98.10(18) 1_554 . ? O5 Mn1 O4 94.35(18) 2_556 . ? O5 Mn1 O4 94.35(18) 1_554 2 ? O5 Mn1 O4 98.10(18) 2_556 2 ? O4 Mn1 O4 163.0(3) . 2 ? O5 Mn1 O1 163.68(18) 1_554 . ? O5 Mn1 O1 99.90(19) 2_556 . ? O4 Mn1 O1 66.27(17) . . ? O4 Mn1 O1 100.08(18) 2 . ? O5 Mn1 O1 99.90(19) 1_554 2 ? O5 Mn1 O1 163.68(18) 2_556 2 ? O4 Mn1 O1 100.08(18) . 2 ? O4 Mn1 O1 66.28(17) 2 2 ? O1 Mn1 O1 79.2(3) . 2 ? O5 Mn1 P1 131.30(13) 1_554 . ? O5 Mn1 P1 98.25(14) 2_556 . ? O4 Mn1 P1 33.32(12) . . ? O4 Mn1 P1 132.39(14) 2 . ? O1 Mn1 P1 32.96(13) . . ? O1 Mn1 P1 89.80(14) 2 . ? O5 Mn1 P1 98.25(14) 1_554 2 ? O5 Mn1 P1 131.30(13) 2_556 2 ? O4 Mn1 P1 132.39(14) . 2 ? O4 Mn1 P1 33.32(12) 2 2 ? O1 Mn1 P1 89.80(14) . 2 ? O1 Mn1 P1 32.96(13) 2 2 ? P1 Mn1 P1 113.69(9) . 2 ? O5 Mn1 NaX 42.73(14) 1_554 . ? O5 Mn1 NaX 42.73(14) 2_556 . ? O4 Mn1 NaX 98.48(13) . . ? O4 Mn1 NaX 98.48(13) 2 . ? O1 Mn1 NaX 140.38(14) . . ? O1 Mn1 NaX 140.38(14) 2 . ? P1 Mn1 NaX 123.16(4) . . ? P1 Mn1 NaX 123.16(4) 2 . ? O5 Mn1 NaX 137.27(14) 1_554 1_545 ? O5 Mn1 NaX 137.27(14) 2_556 1_545 ? O4 Mn1 NaX 81.52(13) . 1_545 ? O4 Mn1 NaX 81.52(13) 2 1_545 ? O1 Mn1 NaX 39.62(14) . 1_545 ? O1 Mn1 NaX 39.62(14) 2 1_545 ? P1 Mn1 NaX 56.84(4) . 1_545 ? P1 Mn1 NaX 56.84(4) 2 1_545 ? NaX Mn1 NaX 180.0 . 1_545 ? O6 Mn2A O6 180.0 4_665 2_546 ? O6 Mn2A OW11 96.5(2) 4_665 3_656 ? O6 Mn2A OW11 83.5(2) 2_546 3_656 ? O6 Mn2A OW11 83.5(2) 4_665 . ? O6 Mn2A OW11 96.5(2) 2_546 . ? OW11 Mn2A OW11 180.0 3_656 . ? O6 Mn2A OW12 91.4(2) 4_665 3_666 ? O6 Mn2A OW12 88.6(2) 2_546 3_666 ? OW11 Mn2A OW12 90.1(2) 3_656 3_666 ? OW11 Mn2A OW12 89.9(2) . 3_666 ? O6 Mn2A OW12 88.6(2) 4_665 1_545 ? O6 Mn2A OW12 91.4(2) 2_546 1_545 ? OW11 Mn2A OW12 89.9(2) 3_656 1_545 ? OW11 Mn2A OW12 90.1(2) . 1_545 ? OW12 Mn2A OW12 180.0 3_666 1_545 ? O2 Mn2B O2 91.2(3) 2_556 . ? O2 Mn2B OW13 85.7(2) 2_556 . ? O2 Mn2B OW13 97.8(2) . . ? O2 Mn2B OW13 97.8(2) 2_556 2_556 ? O2 Mn2B OW13 85.7(2) . 2_556 ? OW13 Mn2B OW13 175.0(3) . 2_556 ? O2 Mn2B OW10 91.9(2) 2_556 2_556 ? O2 Mn2B OW10 171.4(2) . 2_556 ? OW13 Mn2B OW10 90.4(2) . 2_556 ? OW13 Mn2B OW10 86.0(2) 2_556 2_556 ? O2 Mn2B OW10 171.4(2) 2_556 . ? O2 Mn2B OW10 91.9(2) . . ? OW13 Mn2B OW10 86.0(2) . . ? OW13 Mn2B OW10 90.4(2) 2_556 . ? OW10 Mn2B OW10 86.1(3) 2_556 . ? O7 Fe3A O7 180.0(2) 3_566 1_544 ? O7 Fe3A OH9 89.24(19) 3_566 3_565 ? O7 Fe3A OH9 90.76(19) 1_544 3_565 ? O7 Fe3A OH9 90.76(19) 3_566 1_545 ? O7 Fe3A OH9 89.24(19) 1_544 1_545 ? OH9 Fe3A OH9 180.0(5) 3_565 1_545 ? O7 Fe3A O3 84.8(2) 3_566 3 ? O7 Fe3A O3 95.2(2) 1_544 3 ? OH9 Fe3A O3 88.76(19) 3_565 3 ? OH9 Fe3A O3 91.24(19) 1_545 3 ? O7 Fe3A O3 95.2(2) 3_566 . ? O7 Fe3A O3 84.8(2) 1_544 . ? OH9 Fe3A O3 91.24(19) 3_565 . ? OH9 Fe3A O3 88.76(19) 1_545 . ? O3 Fe3A O3 180.0 3 . ? O8 Fe3B O8 180.0(3) 3_566 1_554 ? O8 Fe3B OH9 86.93(19) 3_566 . ? O8 Fe3B OH9 93.07(19) 1_554 . ? O8 Fe3B OH9 93.07(19) 3_566 3_565 ? O8 Fe3B OH9 86.93(19) 1_554 3_565 ? OH9 Fe3B OH9 180.0 . 3_565 ? O8 Fe3B O4 90.00(19) 3_566 3_565 ? O8 Fe3B O4 90.00(19) 1_554 3_565 ? OH9 Fe3B O4 89.82(19) . 3_565 ? OH9 Fe3B O4 90.18(19) 3_565 3_565 ? O8 Fe3B O4 90.00(19) 3_566 . ? O8 Fe3B O4 90.00(19) 1_554 . ? OH9 Fe3B O4 90.18(19) . . ? OH9 Fe3B O4 89.82(19) 3_565 . ? O4 Fe3B O4 180.0 3_565 . ? O3 P1 O2 110.6(3) . . ? O3 P1 O1 108.9(3) . . ? O2 P1 O1 111.5(3) . . ? O3 P1 O4 111.2(3) . . ? O2 P1 O4 113.5(3) . . ? O1 P1 O4 100.7(3) . . ? O3 P1 Mn1 123.0(2) . . ? O2 P1 Mn1 126.3(2) . . ? O1 P1 Mn1 51.0(2) . . ? O4 P1 Mn1 49.63(17) . . ? O3 P1 NaX 62.7(2) . 1_545 ? O2 P1 NaX 136.1(2) . 1_545 ? O1 P1 NaX 47.1(2) . 1_545 ? O4 P1 NaX 108.64(19) . 1_545 ? Mn1 P1 NaX 74.40(6) . 1_545 ? O6 P2 O8 109.5(3) . . ? O6 P2 O7 111.5(3) . . ? O8 P2 O7 111.3(3) . . ? O6 P2 O5 108.6(3) . . ? O8 P2 O5 109.6(3) . . ? O7 P2 O5 106.2(3) . . ? O6 P2 NaX 117.9(2) . 1_556 ? O8 P2 NaX 132.4(2) . 1_556 ? O7 P2 NaX 54.7(2) . 1_556 ? O5 P2 NaX 52.1(2) . 1_556 ? P1 O1 Mn1 96.0(2) . . ? P1 O1 NaX 104.5(3) . 1_545 ? Mn1 O1 NaX 104.1(2) . 1_545 ? P1 O2 Mn2B 143.0(3) . . ? P1 O3 Fe3A 142.4(3) . . ? P1 O3 NaX 88.8(2) . 1_545 ? Fe3A O3 NaX 102.2(2) . 1_545 ? P1 O4 Fe3B 128.6(3) . . ? P1 O4 Mn1 97.0(2) . . ? Fe3B O4 Mn1 128.3(2) . . ? P2 O5 Mn1 129.1(3) . 1_556 ? P2 O5 NaX 98.4(2) . 1_556 ? Mn1 O5 NaX 102.8(2) 1_556 1_556 ? P2 O6 Mn2A 135.2(3) . 2_566 ? P2 O7 Fe3A 134.6(3) . 1_566 ? P2 O7 NaX 95.9(2) . 1_556 ? Fe3A O7 NaX 112.0(2) 1_566 1_556 ? P2 O8 Fe3B 133.5(3) . 1_556 ? Fe3A OH9 Fe3B 127.1(2) 1_565 . ? Fe3A OH9 H9 114(7) 1_565 . ? Fe3B OH9 H9 107(7) . . ? Mn2B OW10 H10A 122(7) . . ? Mn2B OW10 H10B 112(7) . . ? H10A OW10 H10B 111(5) . . ? Mn2A OW11 H11A 120(7) . . ? Mn2A OW11 H11B 84(7) . . ? H11A OW11 H11B 104(5) . . ? Mn2A OW12 H12A 120(7) 1_565 . ? Mn2A OW12 H12B 108(7) 1_565 . ? H12A OW12 H12B 107(5) . . ? Mn2B OW13 H13A 123(6) . . ? Mn2B OW13 H13B 118(6) . . ? H13A OW13 H13B 102(4) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag OH9 H9 OW11 0.82(3) 2.27(4) 3.068(8) 164(10) 4_565 yes OW10 H10A O5 0.80(3) 1.97(4) 2.754(7) 167(10) 2_556 yes OW10 H10B OH9 0.80(3) 2.39(5) 3.136(8) 155(8) . yes OW11 H11A O1 0.82(3) 1.84(3) 2.643(7) 167(9) . yes OW11 H11B OW13 0.82(3) 2.28(5) 3.021(9) 150(8) . yes OW12 H12A O2 0.81(3) 2.01(4) 2.783(8) 160(8) 4_665 yes OW12 H12B OW10 0.80(3) 2.63(8) 3.139(9) 122(8) 3_676 yes OW13 H13B O6 0.83(3) 2.63(9) 3.086(8) 116(8) 4_665 yes OW13 H13B O8 0.83(3) 2.32(3) 3.122(8) 161(7) 4_665 yes _refine_diff_density_max 1.169 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.161